O‹cial Monographs AsolutionofAcebutololHydrochloride(1in20)showsno opticalrotation. Absorptive Ointment Identiˆcation (1) Determinetheabsorptionspectrumofa solution of Acebutolol Hydrochloride in 0.01mol/L 吸水軟膏 hydrochloricacidTS(1in100,000)asdirectedunderUltrav- iolet-visible Spectrophotometry <2.24>, and compare the Method of preparation spectrum with the Reference Spectrum: both spectra exhibit similarintensitiesofabsorption at the same wavelengths. White Petrolatum 400g (2) Determine the infrared absorption spectrum of Cetanol 100g Acebutolol Hydrochloride, previously dried, as directed in White Beeswax 50g the potassium bromide disk method under Infrared Sorbitan Sesquioleate 50g Spectrophotometry <2.25>, and compare the spectrum with Lauromacrogol 5g theReferenceSpectrum:bothspectraexhibitsimilarintensi- EthylParahydroxybenzoateor Methyl ties ofabsorption atthe same wavenumbers. Parahydroxybenzoate 1g (3) A solution of Acebutolol Hydrochloride (1 in 100) ButylParahydroxybenzoateor Propyl responds to the Qualitative Tests <1.09>forchloride. Parahydroxybenzoate 1g Puriˆed Water a su‹cientquantity Melting point <2.60> 141–1459C To make 1000g Purity (1) Heavy metals <1.07>—Proceed with 1.0g of Acebutolol Hydrochloride according to Method 2, and per- MeltWhitePetroleum,Cetanol,WhiteBeeswax,Sorbitan form the test. Prepare the control solution with 1.0mL of SesquioleateandLauromacrogolbyheatingonawaterbath, Standard Lead Solution (notmore than 10ppm). mix and maintain at about 759C. Add Methyl Parahydrox- (2) Arsenic <1.11>—Prepare the test solution with 1.0g ybenzoate or Ethyl Parahydroxybenzoate and Propyl Para- of Acebutolol Hydrochloride according to Method 3, and hydroxybenzoate or Butyl Parahydroxybenzoate to Puriˆed perform the test (not more than 2ppm). Water, dissolve by warming at 809C. Combine both solu- (3) Related substances—Dissolve 40mg of Acebutolol tions,mixtomakeemulsion,cool,andstirthoroughlyuntil Hydrochloridein2mLofmethanol,andusethissolutionas itcongeals. thesamplesolution.Pipet1mLofthesamplesolution,add Description Absorptive Ointment is white in color and is methanol to make exactly 25mL, and pipet 1mL of this lustrous. Ithas a slightly characteristic odor. solution,addmethanoltomakeexactly20mL,andusethis solutionasthestandardsolution.Performthetestwiththese Containers and storage Containers—Tightcontainers. solutions as directed under Thin-layer Chromatography <2.03>. Spot 5mL each of the sample solution and standard Acebutolol Hydrochloride solution on a plate of silica gel for thin-layer chromatography. Develop the plate with the upper layer of a mixtureofwater,1-butanolandaceticacid(100)(5:4:1)toa アセブトロール塩酸塩 distance of about 10cm, and air-dry the plate. Examine under ultraviolet light (main wavelength:365nm):the spots otherthantheprincipalspotfromthesamplesolutionarenot more intense than the spotfrom the standard solution. Loss on drying <2.41> Not more than 1.0z (0.5g, 1059C, 3 hours). C H NO.HCl: 372.89 Residue on ignition <2.44> Not morethan 0.2z(1g). 18 28 2 4 N-s3-Acetyl-4-[(2RS)-2-hydroxy- Assay Weigh accurately about 0.25g of Acebutolol 3-(1-methylethyl)aminopropyloxy]phenyltbutanamide Hydrochloride,previouslydried,dissolvein20mLofacetic monohydrochloride [34381-68-5] acid(100),add80mLofaceticanhydride,andtitrate<2.50> with0.1molWLperchloricacidVS(potentiometrictitration). AcebutololHydrochloride,whendried,containsnot Performablankdetermination,andmakeanynecessarycor- less than 98.0z and not more than 102.0z of rection. C H N O .HCl. 18 28 2 4 Each mL of 0.1molWL perchloric acid VS Description Acebutolol Hydrochloride occurs as white to ＝37.29mg ofC H N O.HCl pale yellowish white crystalsor crystalline powder. 18 28 2 4 It is freely soluble in water, in methanol, in ethanol (95) Containers and storage Containers—Well-closed contain- and in acetic acid (100), and practically insoluble in diethyl ers. ether. 226655 226666 Aceglutamide Aluminum / O‹cial Monographs JP XV ppm). (2) Arsenic <1.11>—Prepare the test solution with 1.0g Aceglutamide Aluminum of Aceglutamide Aluminum according to Method 1, and perform the test (not more than 2ppm). アセグルタミドアルミニウム (3) Relatedsubstances—Dissolve0.10gofAceglutamide Aluminuminthemobilephasetomakeexactly100mL,and use this solution as the sample solution. Pipet 1mL of the sample solution, add the mobile phase to make exactly 100 mL, and use this solution as the standard solution (1). Separately, dissolve 10mg of 2-acetamidoglutarimide in the mobile phase to make exactly 100mL. Pipet 3mL of this solution,addthemobilephasetomakeexactly100mL,and usethissolutionasthestandardsolution(2).Performthetest C H AlN O : 1084.84 35 59 3 10 24 withexactly20mLeachofthesamplesolutionandstandard Pentakis[(2S)-2-acetylamino-4- solutions (1) and (2) as directed under Liquid Chro- carbamoylbutanoato]tetrahydroxotrialuminium matography <2.01> according to the following conditions, [12607-92-0] and determine each peak area by the automatic integration method: the peak area of 2-acetamidoglutarimide from the Aceglutamide Aluminum contains not less than samplesolutionisnotmorethanthatfromthestandardsolu- 85.4z and not more than 87.6z of aceglutamide tion (2), the peak areas other than aceglutamide and 2- (C H N O : 188.18), and not less than 7.0z and not 7 12 2 4 acetamidoglutarimidefromthesamplesolutionarenotmore more than 8.0z of aluminum (Al: 26.98), calculated than 3/10 times the peak area of aceglutamide from the on the dried basis. standard solution (1), and the total of the peak areas other Description Aceglutamide Aluminum occurs as a white than aceglutamide and 2-acetamidoglutarimide from the powder, having astringentbittertaste. sample solution is not more than the peak area of It is freely soluble in water, and practically insoluble in aceglutamidefrom the standard solution (1). ethanol(99.5). Operating conditions— Itdissolves in dilute hydrochloric acid. Detector,column,columntemperature,mobilephase,and Itis hygroscopic. ‰ow rate: Proceed as directed in the operating conditionsin the Assay. Identiˆcation (1) Dissolve 0.03g each of Aceglutamide Time span of measurement: About 3 times as long as the AluminumandAceglutamideReferenceStandardin5mLof retention timeofaceglutamide. water, and use these solutions as the sample solution and System suitability— standard solution. Perform the test with these solutions as Test for required detection: To exactly 5mL of the directedunderThin-layerChromatography<2.03>.Spot5mL standardsolution(1)addthemobilephasetomakeexactly50 eachofthesamplesolutionandstandardsolutiononaplate mL. Conˆrm that the peak area of aceglutamide obtained ofcelluloseforthin-layerchromatography.Developtheplate from20mLofthissolutionisequivalentto7to13zofthat with a mixture of 1-propanol, water and acetic acid (100) of aceglutamide obtained from 20mL of the standard solu- (16:8:1) to a distance of about 10cm, and air-dry the plate. tion. Sprayevenlyasolutionofbromocresolgreeninethanol(95) System performance: Proceed as directed in the system (1in1000),thensprayevenlydilutedammoniasolution(28) suitability in the Assay (1). (1 in 100): the spots from the sample solution and the stan- Systemrepeatability:Whenthetestisrepeated6timeswith dardsolutionshowalightyellowandhavethesameRfvalue. 20mLofthestandardsolution(1)undertheaboveoperating (2) A solution of Aceglutamide Aluminum in dilute conditions,therelativestandarddeviationofthepeakareaof hydrochloric acid(1 in 20)respondstotheQualitativeTests aceglutamideis notmore than 2.0z. <1.09>for aluminum salt. Loss on drying <2.41> Not more than 5.0z (1g, 1309C, Opticalrotation<2.49> [a]20:－5.5–－7.59(2gcalculated D 5hours). on the dried basis,water,50mL,100mm). Assay (1) Aceglutamide—Weigh accurately about 50mg Purity (1) Heavy metals < 1.07 > —Put 1.0g of ofAceglutamideAluminum,dissolveinasuitableamountof Aceglutamide Aluminum in a porcelain crucible, cover the themobilephase,addexactly10mLoftheinternalstandard crucibleloosely,andheatgentlytocarbonize.Aftercooling, solution and the mobile phase to make 50mL, and use this add2mLofnitricacidand1mLofsulfuricacid,heatgently solutionasthesamplesolution.Separately,weighaccurately untilthewhitefumesnomoreevolve,andheattoincinerate about 45mg of Aceglutamide Reference Standard, dissolve at500to6009C.Iftheincinerationisnotaccomplished,add inasuitableamountofthemobilephase,addexactly10mL 2mL of nitric acid and 1mL of sulfuric acid, heat in the of the internal standard solution and the mobile phase to samemannerasabove,thenigniteat500to6009Ctoinciner- make50mL,andusethis solutionasthe standard solution. ate. After cooling, add 2mL of hydrochloric acid, proceed Performthetestwith10mLeachofthesamplesolutionand with this solution according to Method 2, and perform the standardsolutionasdirectedunderLiquidChromatography test. Prepare the control solution as follows: proceed in the <2.01>according to the following conditions, and determine samemannerasthepreparationofthetestsolutionwiththe the ratios, Q and Q , of the peak area of aceglutamide to same amount of the reagents, and add 2.0mL of Standard T S that of theinternal standard. Lead Solution and water to make 50mL (not more than 20 Amount (mg) of aceglutamide (C H N O) 7 12 2 4 JP XV O‹cial Monographs / Acetaminophen 226677 ＝W ×(Q /Q ) crystalline powder. S T S Itisfreelysolubleinmethanolandinethanol(95),sparing- W : Amount(mg)ofAceglutamide Reference Standard S lysolubleinwater,andveryslightly,solubleindiethylether. Internal standard solution—A solution of thymine in It dissolves in sodium hydroxide TS. methanol(1 in 4000). Identiˆcation Determinetheinfraredabsorptionspectraof Operating conditions— Acetaminophen,previouslydried,asdirectedinthepotassi- Detector: An ultraviolet absorption photometer (wave- umbromidediskmethodunderInfraredSpectrophotometry length:210nm). <2.25>, and compare the spectrum with the Reference Spec- Column: A stainless steel column 4.6mm in inside trum or the spectrum of dried Acetaminophen Reference diameterand25cminlength,packedwithoctadecylsilanized Standard: both spectra exhibit similar intensities of absorp- silica gel for liquid chromatography (5mm in particle tion at the samewave numbers. diameter). Column temperature: A constant temperature of about Melting point <2.60> 169–1729C 259C. Purity (1) Chloride < 1.03 > —Dissolve 4.0g of Mobile phase: A mixture of diluted perchloric acid (1 in Acetaminophen in 100mL of water by heating, cool with 1000) and methanol(99:1). shaking in ice water, allow to stand until ordinary tempera- Flowrate:Adjustthe‰owratesothattheretentiontimeof tureisattained,addwatertomake100mL,andˆlter.To25 aceglutamideis about5minutes. mLoftheˆltrateadd6mLofdilutenitricacidandwaterto Systemsuitability— make50mL,andperformthetestusing thissolution asthe System performance: When the procedure is run with test solution. Prepare the control solution with 0.40mL of 10mL of the standard solution under the above operating 0.01molWL hydrochloric acid VS (not more than 0.014z). conditions,aceglutamideandtheinternalstandardareeluted (2) Sulfate <1.14>—To 25mL of the ˆltrate obtained in in this order with the resolution between these peaks being (1)add 1mL of dilute hydrochloric acid and water to make notless than 11. 50mL, and perform the test using this solution as the test Systemrepeatability:Whenthetestisrepeated6timeswith solution.Preparethecontrolsolutionwith0.40mLof0.005 10mL of the standard solution under the above operating molWL sulfuric acid VS (not more than 0.019z). conditions,therelativestandarddeviationoftheratiosofthe (3) Heavy metals <1.07>—Proceed with 2.0g of peakareaofaceglutamidetothatoftheinternalstandardis Acetaminophen according to Method 4, and perform the notmore than 1.0z. test. Prepare the control solution with 2.0mL of Standard (2) Aluminum—Weigh accurately about 3.0g of Lead Solution (not more than 10ppm). Aceglutamide Aluminum, add 20mL of dilute hydrochloric (4) Arsenic <1.11>—Prepare the test solution with 1.0g acid,andheatonawaterbathfor60minutes.Aftercooling, of Acetaminophen according to Method 3,and perform the addwatertomakeexactly200mL.Pipet20mLofthissolu- test(not more than 2ppm). tion,addexactly25mLof0.05mol/Ldisodiumdihydrogen (5) Related substances—Dissolve 50mg of ethylenediamine tetraacetate VS and 20mL of acetic acid- Acetaminophenin1mLofmethanol,addthemobilephase- ammonium acetate buŠer solution, pH4.8, and boil for tomake50mL,andusethissolutionasthesamplesolution. 5 minutes. After cooling, add 50mL of ethanol (95), and Pipet 1mL of the sample solution, add the mobile phase to titrate<2.50>with0.05mol/LzincacetateVSuntilthecolor make exactly 200mL, and use this solution as the standard ofthesolutionchangesfromlightdarkgreentolightred(in- solution.Performthetestwithexactly10mLeachofthesam- dicator:2mLofdithizoneTS).Performablankdetermina- ple solution and standard solution as directed under Liquid tion in the same manner. Chromatography <2.01> according to the following condi- EachmL of 0.05mol/L disodium dihydrogen tions. Determine each peak area of both solutions by the ethylenediamine tetraacetateVS＝1.349mg ofAl automatic integration method: the total area of all peaks otherthanthepeakareaofacetaminophenfromthesample Containers and storage Containers—Tightcontainers. solution is not larger than the peak area of acetaminophen from thestandard solution. Acetaminophen Operating conditions— Detector: An ultraviolet absorption photometer (wavelength: 225nm). Paracetamol Column: A stainless steel column about 4mm in inside diameterand about 15cm in length,packed with octadecyl- アセトアミノフェン silanizedsilicagelforliquidchromatography(5mminparti- cle diameter). Column temperature: A constant temperature of about 409C. Mobile phase: A mixture of 0.05molWL potassium di- C HNO :151.16 8 9 2 hydrogenphosphate, pH 4.7 and methanol(4:1) N-(4-Hydroxyphenyl)acetamide [103-90-2] Flowrate:Adjustthe‰owratesothattheretentiontimeof acetaminophen is about 5 minutes. Acetaminophen, when dried, contains not less than Selection of column: Dissolve 0.01g each of 98.0z of C H NO . 8 9 2 Acetaminophen and p-aminophenol in 1mL of methanol, Description Acetaminophen occurs as white crystals or addthemobilephasetomake50mL,to1mLofthissolution 226688 Acetazolamide / O‹cial Monographs JP XV addthemobilephasetomake10mL.Proceedwith10mLof (2) To 0.02g of Acetazolamide add 2mL of dilute this solution under the above operating conditions, and hydrochloricacid,boilfor10minutes,cool,andadd8mLof calculate the resolution. Use a column giving elution of p- water: this solution responds to the Qualitative Tests <1.09> aminophenol and acetaminophen in this order with the for primary aromatic amines. resolution between these peaksbeing not lessthan 7. (3) To 0.2g of Acetazolamide add 0.5g of granulated Detection sensitivity: Adjust the detection sensitivity so zinc and 5mL of diluted hydrochloric acid (1 in 2): the gas thatthepeakheightofacetaminophenobtainedfrom10mL evolved darkens moistened lead (II) acetatepaper. of the standard solution is about 15zofthefullscale. Purity (1) Clarityandcolorofsolution—Dissolve1.0gof Time span of measurement: About 6 times as long as the Acetazolamide in 10mL of sodium hydroxide TS: the retention time of acetaminophen beginningafterthesolvent solution is clearand colorless to pale yellow. peak. (2) Chloride <1.03>—To 1.5g of Acetazolamide add 75 Loss on drying <2.41> Not more than 0.3z (0.5g, 1059C, mL of water, and warm at 709C for 20 minutes with 2 hours). occasional shaking. After cooling, ˆlter, and to 25mL of theˆltrateadd6mL ofdilutenitricacid andwaterto make Residueon ignition <2.44> Not more than 0.1z(1g). 50mL. Perform the test using this solution as the test solu- Assay Weigh accurately about 20mg each of tion.Preparethecontrolsolutionwith0.20mLof0.01molW Acetaminophen and Acetaminophen Reference Standard, L hydrochloricacid VS (notmore than 0.014z). previously dried, dissolve in 2mL of methanol, and add (3) Sulfate <1.14>—To 25mL of the ˆltrate obtained in water to make exactly 100mL. Pipet 3mL each of these (2)add 1mL of dilute hydrochloric acid and water to make solutions, add water to make exactly 100mL, and use these 50mL. Perform the test using this solution as the test solu- solutions as the sample solution and standard solution, tion.Preparethecontrolsolutionwith0.40mLof0.005mol respectively. Determine the absorbances, A and A , of the WL sulfuric acid VS (notmore than 0.038z). T S sample solution and standard solution at the wavelength of (4) Heavy metals <1.07>—Proceed with 1.0g of maximum absorption at about 244nm as directed under AcetazolamideaccordingtoMethod2,andperformthetest. Ultraviolet-visible Spectrophotometry <2.24>,using water as Prepare the control solution with 2.0mL of Standard Lead the blank. Solution (not more than 20ppm). (5) Silver-reducing substances—Wet 5g of Amount(mg)of CHNO ＝W ×(A /A ) 8 9 2 S T S Acetazolamidewith5mLofaldehyde-freeethanol,andadd W :Amount(mg)of Acetaminophen ReferenceStandard 125mL of water, 10mL of nitric acid and exactly 5mL of S 0.1molWLsilvernitrateVS.Stirfor30minutesbyprotecting Containers and storage Containers—Tightcontainers. from light, ˆlter through a glass ˆlter (G3), and wash the Storage—Light-resistant. residueontheglassˆlterwithtwo10-mLportionsofwater. Combine the ˆltrate with the washings, to the solution add Acetazolamide 5mLofferricammoniumsulfaceTS,andtitrate<2.50>with 0.1molWL ammoniumthiocyanate VS:notless than 4.8mL of 0.1molWL ammonium thiocyanate VS is consumed. アセタゾラミド Loss on drying <2.41> Not more than 0.5z (0.5g, 1059C, 3 hours). Residue on ignition <2.44> Not morethan 0.1z(0.5g). Assay Weigh accurately about 0.15g of Acetazolamide, and dissolve in 400mL of waterin a waterbath byheating. After cooling, add water to make exactly 1000mL. Pipet C4H6N4O3S2:222.25 5mL of the solution, add 10mL of 1molWL hydrochloric N-(5-Sulfamoyl-1,3,4-thiadiazol-2-yl)acetamide [59-66-5] acidTS,andthenaddwatertomakeexactly100mL.Deter- minetheabsorbanceAofthissolutionatthewavelengthof Acetazolamidecontainsnotlessthan98.0zandnot maximum absorption at about 265nm as directed under more than 102.0z of C H N O S , calculated on the 4 6 4 3 2 Ultraviolet-visible Spectrophotometry <2.24>. dried basis. Description Acetazolamide occurs as a white to pale Amount(mg)of C4H6N4O3S2＝(A/474)×200,000 yellowishwhite,crystallinepowder.Itisodorless,andhasa slight bitter taste. Containers and storage Containers—Well-closed contain- Itisslightlysolubleinethanol(95),veryslightlysolublein ers. water, and practically insolublein diethyl ether. Storage—Light-resistant. Melting point: about2559C (with decomposition). Identiˆcation (1) To0.1gofAcetazolamideadd5mLof Acetic Acid sodiumhydroxideTS,thenadd5mLofasolutionof0.1gof hydroxylammonium chloride and 0.05g of copper (II) 酢酸 sulfate pentahydrate in 10mL of water:a lightyellow color develops.Thenheatthissolutionfor5minutes:adeepyellow coloris produced gradually. Acetic Acid contains not less than 30.0wWvz and JP XV O‹cial Monographs / Acetohexamide 226699 not more than 32.0wWvz of C H O : 60.05. 2 4 2 Purity (1) Chloride—To 10mL of Glacial Acetic Acid Description AceticAcidisaclear,colorlessliquid.Ithasa addwatertomake100mL,andusethissolutionasthesam- pungent, characteristicodor and an acid taste. plesolution.To10mLofthesamplesolutionadd5dropsof It is miscible with water, with ethanol (95) and with silvernitrate TS:no opalescence isproduced. glycerin. (2) Sulfate—To10mLofthesamplesolutionobtainedin Speciˆc gravity d20: about1.04 (1) add 1mL of barium chloride TS: no turbidity is 20 produced. Identiˆcation AceticAcidchangesbluelitmuspapertored, (3) Heavy metals <1.07>—Evaporate 2.0mL of Glacial and responds to the QualitativeTests <1.09>foracetate. AceticAcidonawaterbathtodryness.Dissolvetheresidue Purity (1) Chloride—To20mLofAceticAcidadd40mL in 2mL ofdiluteaceticacid and waterto make 50mL, and ofwater,andusethissolutionasthesamplesolution.To10 performthetestusingthissolutionasthetestsolution.Pre- mLofthesamplesolutionadd5dropsofsilvernitrateTS:no parethecontrolsolutionwith2.0mLofStandardLeadSolu- opalescence is produced. tionbyadding2.0mLofdiluteaceticacidandwatertomake (2) Sulfate—To10mLofthesamplesolutionobtainedin 50mL (notmore than 10ppm). (1) add 1mL of barium chloride TS: no turbidity is (4) Potassium permanganate-reducing substances—To produced. 20mLofthesamplesolutionobtainedin(1)add0.10mLof (3) Heavy metals <1.07>—Evaporate 10mL of Acetic 0.1molWL potassium permanganate VS: the red color does Acidonawaterbathtodryness,andtotheresidueadd2mL notdisappear within 30minutes. of diluteacetic acid and waterto make 50mL. Perform the (5) Non-volatile residue—Evaporate 10mL of Glacial testwiththissolutionasthetestsolution.Preparethecontrol AceticAcidonawaterbathtodryness,anddryat1059Cfor solutionwith3.0mLofStandardLeadSolutionbyadding2 1hour: the mass ofthe residueis notmore than 1.0mg. mLofdiluteaceticacidandwatertomake50mL(notmore Assay Place10mLofwaterinaglass-stoppered‰ask,and than 3ppm). weigh accurately. Add about 1.5g of Glacial Acetic Acid, (4) Potassium permanganate-reducing substances—To weighaccuratelyagain,thenadd30mLofwater,andtitrate 20mLofthesamplesolutionobtainedin(1)add0.02molWL <2.50>with1molWLsodiumhydroxideVS(indicator:2drops potassium permanganate VS: the red color does not disap- of phenolphthalein TS). pearwithin 30 minutes. (5) Non-volatile residue—Evaporate 30mL of Acetic Each mL of1molWL sodium hydroxide VS Acidonawaterbathtodryness,anddryat1059Cfor1hour: ＝60.05mg of C HO 2 4 2 the massofthe residueis notmore than 1.0mg. Containers and storage Containers—Tightcontainers. Assay Measureexactly5mLofAceticAcid,add30mLof water,andtitrate<2.50>with1molWLsodiumhydroxideVS Acetohexamide (indicator:2drops of phenolphthalein TS). Each mL of1molWL sodium hydroxide VS アセトヘキサミド＝60.05mg of C HO 2 4 2 Containers and storage Containers—Tightcontainers. Glacial Acetic Acid 氷酢酸 C H NOS:324.40 15 20 2 4 4-Acetyl-N-(cyclohexylcarbamoyl)benzenesulfonamide C HO :60.05 [968-81-0] 2 4 2 Acetic acid [64-19-7] Acetohexamide, when dried, contains not less than Glacial Acetic Acid contains not less than 99.0z of 98.0z and not more than 101.0z of C15H20N2O4S. C H O . 2 4 2 Description Acetohexamide occurs as a white to yellowish Description GlacialAceticAcidisaclear,colorless,volatile whitepowder. liquid, or colorless or white, crystalline masses. It has a It is freely soluble in N,N-dimethylformamide, sparingly pungent, characteristicodor. solubleinacetone,slightlysolubleinmethanolandinethanol Itismisciblewithwater,withethanol(95)andwithdiethyl (99.5), and practically insoluble in water. ether. Melting point: about 1859C (with decomposition). Boiling point:about 1189C Identiˆcation (1) Dissolve0.10gofAcetohexamidein100 Speciˆc gravity d20: about1.049 20 mLofmethanol.To 5mLofthesolutionadd 20mL of0.5 Identiˆcation A solution of Glacial Acetic Acid (1 in 3) mol/LhydrochloricacidTSand75mLofmethanol,anduse changes blue litmus paper to red, and responds to the thesolutionasthesamplesolution(1).Determinetheabsorp- Qualitative Tests <1.09>for acetate. tion spectrum of the sample solution (1) as directed under Ultraviolet-visible Spectrophotometry <2.24>, using Congealing point<2.42> Not below 14.59C. methanol as the blank, and compare the spectrum with the 227700 Acetohexamide / O‹cial Monographs JP XV ReferenceSpectrum1:bothspectraexhibitsimilarintensities 2109C. ofabsorptionatthesamewavelengths.Separately,toexactly Carriergas:Helium 10mL of the sample solution (1) add methanol to make ex- Flowrate:Adjustthe‰owratesothattheretentiontimeof actly50mL,andusethesolutionasthesamplesolution(2). cyclohexylamine is about 4 minutes. Determinetheabsorptionspectrumofthesamplesolution(2) Splitratio:1:1 as directed under Ultraviolet-visible Spectrophotometry System suitability— <2.24>, using methanol as the blank, and compare the spec- Systemperformance:Whentheprocedureisrunwith2mL trum with the Reference Spectrum 2: both spectra exhibit of the standard solution under the above operating similarintensitiesof absorption at the samewavelengths. conditions, the number of theoretical plates of the peak of (2) Determine the infrared absorption spectrum of cyclohexylamine is notless than 8000. Acetohexamide, previously dried, as directed in the potassi- Systemrepeatability:Whenthetestisrepeated6timeswith umbromidediskmethodunderInfraredSpectrophotometry 2mLofthestandardsolutionundertheaboveoperatingcon- <2.25>, and compare the spectrum with the Reference Spec- ditions,therelativestandarddeviationofthepeakareaofcy- trum:bothspectraexhibitsimilarintensitiesofabsorptionat clohexylamine is not morethan 5z. the samewave numbers. (ii) Dicyclohexylurea—Dissolve exactly 1.0g of Aceto- hexamide in exactly 10mL of 0.5mol/L sodium hydroxide Purity (1) Chloride <1.03>—Dissolve 1.5g of Acetohex- TS,addexactly20mLofmethanol,shake,thenaddexactly5 amidein40mLofN,N-dimethylformamide,add6mLofdi- mL of diluted hydrochloric acid (1 in 10), shake vigorously lutenitricacidandN,N-dimethylformamidetomake50mL. for 15 minutes, and centrifuge. Filter 10mL or more of the Performthetestusingthissolutionasthetestsolution.Pre- supernatant liquid through a membrane ˆlter with pore size parethecontrolsolutionasfollows:to0.45mLof0.01molW of not larger than 0.5mm. Discard the ˆrst 5mL of the L hydrochloric acid VS add 6mL of dilute nitric acid and ˆltrate,andusethesubsequentˆltrateasthesamplesolution. N,N-dimethylformamide to make 50mL (not more than Separately, dissolve exactly 50mg of dicyclohexylurea in 0.011z). methanol to make exactly 100mL. Pipet 2mL of this solu- (2) Sulfate <1.14>—Dissolve 2.0g of Acetohexamide in tion,andaddmethanoltomakeexactly100mL.Pipet20mL 40mL of N,N-dimethylformamide, and add 1mL of dilute of this solution, add exactly 10mL of 0.5mol/L sodium hydrochloric acid and N,N-dimethylformamide to make 50 hydroxide TS, shake, then add exactly 5mL of diluted mL.Performthetestusingthissolutionasthetestsolution. hydrochloricacid(1in10),shake,andusethissolutionasthe Preparethecontrolsolutionasfollows:to0.40mLof0.005 standard solution. Perform the test with exactly 50mL each molWL sulfuric acid VS add 1mL of dilute hydrochloric ofthesamplesolutionandstandardsolutionasdirectedun- acidandN,N-dimethylformamidetomake50mL(notmore der Liquid Chromatography <2.01> according to the follow- than 0.010z). ing conditions, and determine the peak area of dicyclohex- (3) Heavy metals <1.07>—Proceed with 1.0g of Aceto- ylureabytheautomaticintegrationmethod:thepeakareaof hexamideaccordingtoMethod2,andperformthetest.Pre- dicyclohexylureaisnotmorethanthatwiththestandardso- pare the control solution with 2.0mL of Standard Lead lution. Solution (not more than 20ppm). Operating conditions— (4) Relatedsubstances(i)Cyclohexylamine—Dissolveex- Detector: An ultraviolet absorption photometer actly1.0gofAcetohexamidein exactly30mLof0.5mol/L (wavelength: 210nm). sodium hydroxide TS, add exactly 5mL of hexane, shake Column: A stainless steel column 4.6mm in inside vigorouslyfor60minutes,allowtostandfor5minutes,and diameterand25cminlength,packedwithoctadecylsilanized use the upper layer as the sample solution. Separately, dis- silica gel for liquid chromatography (5mm in particle di- solveexactly50mgofcyclohexylaminein0.5mol/Lsodium ameter). hydroxideTStomakeexactly50mL.Pipet2mLofthissolu- Column temperature: A constant temperature of about tion, and add 0.5mol/L sodium hydroxide TS to make ex- 259C. actly300mL.Pipet30mLofthissolution,addexactly5mL Mobilephase:Dissolve0.5gofsodiumhydroxidein1000 of hexane, shake vigorously for 60 minutes, allow to stand mL of 0.05mol/L sodium dihydrogen phosphate TS, and for 5 minutes,and use the upper layer as the standard solu- adjust the pH to 6.5 with 0.5mol/L sodium hydroxide TS. tion. Perform the test with exactly 2mL each of the sample To 500mL ofthis solution add 500mL of acetonitrile. solution and standard solution as directed under Gas Chro- Flowrate:Adjustthe‰owratesothattheretentiontimeof matography <2.02> according to the following conditions, dicyclohexylurea is about10 minutes. anddeterminethepeakareaofcyclohexylaminebytheauto- System suitability— maticintegrationmethod:thepeakareaofcyclohexylamine System performance: When the procedure is run with isnot morethan that with thestandard solution. 50mL of the standard solution under the above operating Operating conditions— conditions, the number of theoretical plates of the peak of Detector: Ahydrogen ‰ame-ionization detector. dicyclohexylurea is notless than 10,000. Column:Afused-silicacolumn0.53mmininsidediameter Systemrepeatability:Whenthetestisrepeated6timeswith and30minlength,coatedtheinnersurfacewithmethylsili- 50mL of the standard solution under the above operating cone polymer for gaschromatography 1.5mm in thickness. conditions,therelativestandarddeviationofthepeakareaof Column temperature: A constant temperature of about dicyclohexylurea is notmore than 2.0z. 909C. (iii) Other related substances—Dissolve 0.10g of Aceto- Injection port temperature: A constant temperature of hexamide in 10mL of acetone, and use this solution as the about1509C. samplesolution.Pipet1mLofthesamplesolution,andadd Detector temperature: A constant temperature of about acetone to makeexactly 20mL. Pipettwo 1mL portions of JP XV O‹cial Monographs / Acetylcholine Chloride for Injection 227711 thissolution,addacetonetomakeexactly10mLand25mL, It isextremely hygroscopic. respectively,andusethesesolutionsasthestandardsolution Identiˆcation (1) Determine the infrared absorption (1)andthestandardsolution(2).Performthetestwiththese spectrumofAcetylcholineChlorideforInjection,previously solutions as directed under Thin-layer Chromatography dried, as directed in the potassium bromide disk method <2.03>.Spot10mLeachofthesamplesolutionandstandard under Infrared Spectrophotometry <2.25>, and compare the solutions (1) and (2) on a plate of silica gel with ‰uorescent spectrum with the Reference Spectrum: both spectra exhibit indicator for thin-layer chromatography. Develop the plate similarintensitiesofabsorption at the same wave numbers. withamixtureofethylacetate,methanol,ammoniasolution (2) A solution of Acetylcholine Chloride for Injection (28)andcyclohexane(6:2:1:1)toa distanceofabout10cm, (1in10)respondstotheQualitativeTests<1.09>(2)forchlo- and air-dry the plate. Examine under ultraviolet light (main ride. wavelength:254nm):thespotsotherthantheprincipalspot fromthesamplesolutionarenotmoreintensethanspotfrom Melting point <2.60> 149–1529C. Seal Acetylcholine thestandardsolution(1),andthenumberofthemwhichare Chloride for Injection in a capillary tube for melting point moreintense than the spotfrom the standard solution (2)is immediatelyafterdryingbothofthesampleandthetubeat notmore than 4. 1059C for 3 hours, and determine the melting point. Loss on drying <2.41> Not more than 1.0z (1g, 1059C, Purity (1) Clarityandcolorofsolution—Dissolve1.0gof 4 hours). Acetylcholine Chloride for Injection in 10mL of water: the solution is clearand colorless. Residueon ignition <2.44> Not more than 0.1z(1g). (2) Acidity—Dissolve 0.10g of Acetylcholine Chloride Assay Weigh accurately about 0.3g of Acetohexamide, for Injection in 10mL of freshly boiled and cooled water, previously dried, dissolve in 30mL of N,N-dimethylfor- and add 1 drop of bromothymol blue TS, and 0.30mL of mamide,add10mLofwater,andtitrate<2.50>with0.1mol 0.01molWL sodium hydroxide VS: the solution is blue in WLsodiumhydroxideVS(potentiometrictitration).Perform color. ablankdeterminationusingasolutionpreparedbyadding19 (3) Heavy metals <1.07>—Proceed with 2.0g of Acetyl- mL of water to 30mL of N,N-dimethylformamide, and choline Chloride for Injection according to Method 1, and make any necessary correction. performthetest.Preparethecontrolsolutionwith2.0mLof Standard Lead Solution (notmore than 10ppm). Each mL of0.1molWL sodium hydroxide VS ＝32.44mg ofC H N OS Loss on drying <2.41> Not more than 1.0z (1g, 1059C, 3 15 20 2 4 hours). Containers and storage Containers—Well-closed containers. Residue on ignition <2.44> Not morethan 0.1z(1g). Assay (1) Acetylcholine chloride—Weigh accurately the Acetylcholine Chloride for contentsofnotlessthan10AcetylcholineChlorideforInjec- tions.Weighaccuratelyabout0.5gofthecontents,dissolve Injection in15mLofwater,thenaddexactly40mLof0.1molWLsodi- umhydroxideVS,stopperloosely,andheatonawaterbath 注射用アセチルコリン塩化物 for30minutes.Coolquickly,andtitrate<2.50>theexcessso- diumhydroxidewith0.05molWLsulfuricacidVS(indicator: 3dropsofphenolphthaleinTS).Performablankdetermina- tion. Each mL of 0.1molWL sodium hydroxide VS ＝18.17mg ofC H ClNO 7 16 2 C H ClNO :181.66 7 16 2 2-Acetoxy-N,N,N-trimethylethylaminium chloride (2) Chlorine—Titrate<2.50>thesolution,whichhasbeen [60-31-1] titrated in (1),with 0.1molWL silver nitrateVS (indicator:3 drops of ‰uorescein sodium TS). AcetylcholineChlorideforInjectionisapreparation Each mL of0.1molWL silver nitrate VS for injection which is dissolved before use. ＝3.545mg of Cl It contains not less than 98.0z and not more than 102.0z of acetylcholine chloride (C H ClNO ), and Containers and storage Containers—Hermeticcontainers. 7 16 2 notlessthan19.3zandnotmorethan19.8zofchlo- rine (Cl: 35.45), calculated on the dried basis. Itcontainsnotlessthan93zandnotmorethan107 z of the labeled amount of acetylcholine chloride (C H ClNO ). 7 16 2 Method of preparation Prepare as directed under Injec- tions. Description Acetylcholine Chloride for Injection occurs as white crystals or crystallinepowder. It is very soluble in water, and freely soluble in ethanol (95). 227722 Aclarubicin Hydrochloride / O‹cial Monographs JP XV Purity (1) Clarity and color of solution－Dissolve 0.10g Aclarubicin Hydrochloride ofAclarubicinHydrochloridein10mLofwater:thesolution is clear and yellow to pale orange-yellow. (2) Heavymetals<1.07>—Proceedwith1.0gofAclarubi- アクラルビシン塩酸塩 cin Hydrochloride according to Method 2, and perform the test. Prepare the control solution with 2.0mL of Standard Lead Solution (not more than 20ppm). (3) Related substances—Dissolve 10mg of Aclarubicin Hydrochloride in 10mL of the mobile phase, and use this solutionasthesamplesolution.Performthetestwith20mL of the sample solution as directed under Liquid Chro- matography <2.01> according to the following conditions, and determine each peak area by the automatic integration method. Calculate the amount of the related substances by the area percentage method: the amount of aklavinone havingtherelativeretentiontimeofabout0.6toaclarubicin isnotmorethan0.2z,aclacinomycinL1havingtherelative retention timeofabout0.75to aclarubicinisnotmore than 0.5z, 1-deoxypyrromycin having the relative retention time of about 1.7 to aclarubicin is not more than 1.5z and C H NO .HCl: 848.33 aclacinomycinS1havingtherelativeretentiontimeofabout 42 53 15 Methyl (1R,2R,4S)-4-s2,6-dideoxy-4-O-[(2R,6S)-6- 2.3 to aclarubicin is not more than 0.5z, and the total methyl-5-oxo-3,4,5,6-tetrahydro-2H-pyran-2-yl]- amount of the peaks other than aclarubicin and the peaks a-L-lyxo-hexopyranosyl-(1ª4)-2,3,6-trideoxy-3- mentionedaboveisnotmorethan1.0zofthepeakareaof dimethylamino-a-L-lyxo-hexopyranosyloxyt-2-ethyl-2,5,7- aclarubicin. trihydroxy-6,11-dioxo-1,2,3,4-tetrahydrotetracene- Operating conditions— 1-carboxylate monohydrochloride [75443-99-0] Detector: A visible absorption photometer (wavelength: 436nm). Aclarubicin Hydrochloride is the hydrochloride of Column: A stainless steel column 3.9mm in inside an anthracycline substance having antitumor activity diameterand30cminlength,packedwithsilicagelforliquid produced by the growth of Streptomyces galilaeus. chromatography (10mm in particle diameter). It contains not less than 920mg (potency) and not Column temperature: A constant temperature of about more than 975mg (potency) per mg, calculated on the 259C. anhydrous basis. The potency of Aclarubicin Mobilephase:Amixtureofchloroform,methanol,acetic Hydrochloride is expressed as mass (potency) of acid (100),waterand triethylamine (6800:2000:1000:200:1). aclarubicin (C H NO : 811.87). Flowrate:Adjustthe‰owratesothattheretentiontimeof 42 53 15 aclarubicin isabout 5minutes. Description Aclarubicin Hydrochloride occurs as a yellow Timespanofmeasurement:Aslongasabout4timesofthe to pale orange-yellow powder. retention time of aclarubicin beginning after the solvent It is very soluble in chloroform and in methanol, freely peak. soluble in water,and slightly soluble in ethanol(95). System suitability— Identiˆcation (1) Determinetheabsorptionspectrumofa Test for required detectability: Pipet 1mL of the sample solution of Aclarubicin Hydrochloride in diluted methanol solution,addthemobilephasetomakeexactly100mL,and (4 in 5) (3 in 100,000) as directed under Ultraviolet-visible use this solution as the solution for system suitability test. Spectrophotometry <2.24>, and compare the spectrum with Pipet1mLofthesolutionforsystemsuitabilitytest,andadd theReferenceSpectrum:bothspectraexhibitsimilarintensi- the mobile phase to make exactly 10mL. Conˆrm that the tiesofabsorption at the same wavelengths. peakareaofaclarubicinobtainedfrom20mLofthissolution (2) Determine the infrared absorption spectrum of isequivalentto7to13zofthatfrom20mL ofthesolution Aclarubicin Hydrochloride as directed in the potassium for system suitability test. bromide disk method under Infrared Spectrophotometry System performance: Dissolve 5mg of Aclarubicin <2.25>, and compare the spectrum with the Reference Hydrochloridein10mLof0.1mol/LhydrochloricacidTS, Spectrum:both spectra exhibit similar intensities of absorp- andallowtostandfor60minutes.To1.0mLofthissolution tion at the same wave numbers. add 1.0mL of 0.2mol/L sodium hydroxide TS, 1.0mL of (3) AsolutionofAclarubicinHydrochlorideinmethanol phosphate buŠer solution, pH8.0 and 1.0mL of chlo- (1 in 200) responds to the Qualitative Tests <1.09> (2) for roform, shake vigorously, and take the chloroform layer. chloride. When the procedure is run with 20mL of the chloroform under the above operating conditions, aclarubicin and 1- Opticalrotation<2.49>[a]20:－146–－1629(50mgcalculat- D deoxypyrromycinareelutedinthisorderwiththeresolution ed on the anhydrous basis,water, 10mL, 100 mm). between these peaks being notless than 3.0. pH <2.54> The pH of a solution obtained by dissolving Systemrepeatability:Whenthetestisrepeated5timeswith 0.05g of Aclarubicin Hydrochloride in 10mL of water is 20mL of the sample solution under the above operating between 5.5 and 6.5. conditions,therelativestandarddeviationofthepeakareaof JP XV O‹cial Monographs / Compound Acrinol and Zinc Oxide Oil 227733 aclarubicin is notmore than 2.0z. and 2.5mL ofacetic acid (100),and use thissolution asthe standard solution. Perform the test with these solutions as Water <2.48> Not more than 3.5z (0.1g, volumetric directedunderThin-layerChromatography<2.03>.Spot5mL titration, direct titration). eachofthesamplesolutionandstandardsolutiononaplate Residueon ignition <2.44> Not more than 0.1z(1g). ofsilicagelforthin-layerchromatography.Developtheplate withamixtureof2-propanolandaceticacid(100)(9:1)toa Assay Weigh accurately an amount of Aclarubicin distanceofabout10cm,andair-drytheplate.Examineun- Hydrochloride,equivalenttoabout20mg(potency),anddis- der ultraviolet light (main wavelength: 365nm): the spots solve in diluted methanol (4 in 5) to make exactly 100mL. fromthesamplesolutionandstandardsolutionexhibitablue Pipet15mLofthissolution,adddilutedmethanol(4in5)to ‰uorescence and show the same Rfvalue. make exactly 100mL, and use this solution as the sample solution. Separately, weigh accurately an amount of Containers and storage Containers—Tightcontainers. Aclarubicin Reference Standard, equivalent to about 20mg Storage—Light-resistant. (potency),add0.6mLofdilutedhydrochloricacid(1in250) anddilutedmethanol(4in5)tomakeexactly100mL.Pipet Compound Acrinol and Zinc Oxide 15mLofthissolution,adddilutedmethanol(4in5)tomake exactly 100mL, and use this solution as the standard solu- Oil tion.Performthetestwiththesamplesolutionandstandard solution as directed under Ultraviolet-visible Spectrophoto- 複方アクリノール・チンク油 metry<2.24>,anddeterminetheabsorbances,A andA ,at T S 433nm. Method of preparation Amount[mg (potency)] of aclarubicin (C H NO ) 42 53 15 ＝WS×(AT/AS)×1000 Acrinol, very ˆnely powdered 10g Zinc Oxide Oil 650g W : Amount [mg (potency)] of Aclarubicin Reference S EthylAminobenzoate, ˆnely powdered 50g Standard White Beeswax 20g Containers and storage Containers—Tightcontainers. Hydrophilic Petrolatum 270g Storage—Light-resistantand at59C or below. To make 1000g Prepare by mixing the above ingredients. Acrinol and Zinc Oxide Oil Description CompoundAcrinolandZincOxideOilislight yellow to yellow in color. アクリノール・チンク油 Identiˆcation (1) Shake well 1g of Compound Acrinol and Zinc Oxide Oil with 10mL of diethyl ether, 2mL of Method of preparation aceticacid(100)and10mLofwater,andseparatethewater Acrinol, very ˆnely powdered 10g layer.Shake the layer with 5mL ofhydrochloricacid and 2 ZincOxide Oil 990g to 3 drops of sodium nitrite TS, and allow to stand: a dark red color is produced (acrinol). To make 1000g (2) Place1gofCompoundAcrinolandZincOxideOilin Prepare by mixing theabove ingredients. acrucible,meltbywarming,heat,graduallyraisingthetem- peratureuntilthemassisthoroughlycharred,andthenignite Description Acrinol and Zinc Oxide Oil is a yellowish strongly: a yellow color is produced, and disappears on white,slimysubstance.Separationofapartofitsingredients cooling. To the residue add 10mL of water and 5mL of occurs on prolonged standing. dilutehydrochloricacid,shakewell,andˆlter.Totheˆltrate Identiˆcation (1) Shake well 1g of Acrinol and Zinc add 2 to 3 drops of potassium hexacyanoferrate (II) TS: a Oxide Oil with 10mL of diethyl ether, 2mL of acetic acid whiteprecipitate is produced (zinc oxide). (100) and 10mL of water, and separate the water layer. (3) Shake well 0.2g of Compound Acrinol and Zinc Shake the layer with 5mL of hydrochloric acid and 2 to 3 OxideOilwith20mLofethanol(95)and1mLofaceticacid drops of sodium nitrite TS, and allow to stand: a dark red (100), centrifuge, ˆlter, and use the ˆltrate as the sample coloris produced (acrinol). solution. Separately, dissolve 5mg of acrinol and 25mg of (2) Place1gofAcrinolandZincOxideOilinacrucible, ethylaminobenzoatein50mLofethanol(95)andin2.5mL melt by warming, heat, gradually raising the temperature of acetic acid (100), respectively, and use both solutions as untilthemassisthoroughlycharred,andthenignitestrongly: thestandardsolutions(1)and(2).Performthetestwiththese ayellowcolorisproduced,anddisappearsoncooling.Tothe solutionsasdirectedunderThin-layerChromatography<2.03 residueadd10mLofwaterand5mLofdilutehydrochloric >.Spot5mLeachofthesamplesolutionand standard solu- acid,ˆlterafterthoroughshaking,andtotheˆltrateadd2to tions on a plate of silica gel with ‰uorescent indicator for 3 drops of potassium hexacyanoferrate (II) TS: a white thin-layerchromatography.Developtheplatewithamixture precipitateis formed (zinc oxide). of 2-propanol and acetic acid (100) (9:1) to a distance of (3) Shake well 0.2g of Acrinol and Zinc Oxide Oil with about10cm,andair-drytheplate.Examineunderultraviolet 20mL of ethanol (95) and 1mL of acetic acid (100), cen- light (main wavelength: 365nm): the spots from the sample trifuge, ˆlter, and use the ˆltrate as the sample solution. solutionandstandardsolution(1)exhibitablue‰uorescence, Separately,dissolve5mgofacrinolin50mLofethanol(95) andshowthesameRfvalue.Alsoexamineunderultraviolet 227744 Acrinol and Zinc Oxide Ointment / O‹cial Monographs JP XV light (main wavelength: 254nm): the spots from the sample solutionandstandardsolution(2)exhibitapurplecolor,and show the same Rfvalue. Acrinol Hydrate Containers and storage Containers—Tightcontainers. Ethacridine Lactate Storage—Light-resistant. アクリノール水和物 Acrinol and Zinc Oxide Ointment アクリノール・亜鉛華軟膏 Method of preparation C H NO.C H O.HO: 361.39 15 15 3 3 6 3 2 2-Ethoxy-6,9-diaminoacridine monolactate monohydrate Acrinol, very ˆnely powdered 10g ZincOxide Ointment 990g [1837-57-6] To make 1000g Acrinol Hydrate contains not less than 98.5z and Prepare as directed under Ointments, with the above notmorethan101.0zofacrinol(C15H15N3O.C3H6O3: ingredients. 343.38), calculated on the anhydrous basis. Description Acrinol and Zinc oxide Ointment is yellow in Description AcrinolHydrateoccursasayellow,crystalline color. powder. Itissparinglysolubleinwater,inmethanolandinethanol Identiˆcation (1) Shake 0.5g of Acrinol and Zinc Oxide (99.5). Ointment with 5mL of diethyl ether, 5mL of dilute Melting point: about 2459C (with decomposition). hydrochloricacidand2to3dropsofsodiumnitriteTS,and ThepH of a solution of AcrinolHydrate(1 in 100)is be- allow to stand: a dark red color develops in the water layer tween 5.5 and 7.0. (acrinol). (2) Ignite 0.5g of Acrinol and Zinc Oxide Ointment to Identiˆcation (1) Determinetheabsorptionspectrumofa char,anddissolvetheresiduein5mLofdilutehydrochloric solutionofAcrinolHydrate(3in250,000)asdirectedunder acid:thesolutionrespondstotheQualitativeTests<1.09>for Ultraviolet-visible Spectrophotometry <2.24>, and compare zinc salt. the spectrum with the Reference Spectrum:both spectra ex- (3) Shake0.5gofAcrinolandZincOxideOintmentwith hibit similar intensities of absorption at the same 5mLofdiethylether,1mLofaceticacid(100)and5mLof wavelengths. water,separatethewaterlayer,andusethewaterlayerasthe (2) Determine the infrared absorption spectrum of sample solution. Dissolve 5mg of acrinol in 1mL of acetic Acrinol Hydrate as directed in the potassium bromide disk acid (100) and 5mL of water, and use this solution as the methodunderInfraredSpectrophotometry<2.25>,andcom- standard solution. Perform the test with these solutions as parethespectrumwiththeReferenceSpectrum:bothspectra directedunderThin-layerChromatography<2.03>.Spot5mL exhibit similar intensities of absorption at the same wave eachofthesamplesolutionandstandardsolutiononaplate numbers. ofsilicagelforthin-layerchromatography.Developtheplate (3) To 5mL of a solution of Acrinol Hydrate (1 in 100) with a mixture of diethyl ether, ethanol (95) and acetic acid add 5mL of dilute sulfuric acid, shake well, allow to stand (100)(40:10:1)toadistanceofabout10cm,andair-drythe for about 10 minutes at room temperature, and ˆlter: the plate.Examineunderultravioletlight(mainwavelength:365 ˆltrate responds to the QualitativeTests <1.09>forlactate. nm):thespotsfromthesamplesolutionandthestandardso- Purity (1) Chloride<1.03>—Dissolve1.0gofAcrinolHy- lution exhibit a blue ‰uorescence and show the same Rf drate in 80mL of water by warming on a water bath, cool, value. and add 10mL of sodium hydroxide TS and water to make Containers and storage Containers—Tightcontainers. 100mL.Shakewell,allow tostandfor30minutes,ˆlter,to Storage—Light-resistant. 40mLoftheˆltrateadd7mLofdilutenitricacidandwater to make 50mL, and perform the test using this solution as thetestsolution.Prepare50mLofthecontrolsolutionwith 4mL of sodium hydroxide TS, 7mL of dilute nitric acid, 0.30mL of 0.01mol/L hydrochloric acid VS and su‹cient water (not more than 0.026z). (2) Heavy metals <1.07>—Proceed with 1.0g of Acrinol Hydrate according to Method 2, and perform the test. Pre- parethecontrolsolutionwith2.0mLofStandardLeadSolu- tion (notmore than 20ppm). (3) Volatile fatty acids—Dissolve 0.5g of Acrinol Hy- drateinamixtureof20mLofwaterand5mLofdilutesul- furicacid,shakewell,ˆlter,andheattheˆltrate:noodorof volatile fatty acidsis perceptible. (4) Related substances—Dissolve 10mg of Acrinol Hy-

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